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Method for preparing vinyl amine

A technology of ethylene amine and ethanolamine sulfate, applied in the preparation of amino compounds from amines, organic chemistry, etc., can solve the problems of product structure and performance changes, easy to be destroyed, etc., and achieve the effect of low cost and high yield

Inactive Publication Date: 2013-05-08
TIANJIN DEK CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Vinylamine itself has high activity, and the existing process is easily destroyed during the reaction process, resulting in changes in product structure and performance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Esterification

[0022] Add 497.84g of 103% fuming sulfuric acid to the reactor, cool the external bath, add 61.0g of 100% ethanolamine in 35 minutes under the condition that the temperature is less than 30℃, heat up to 40℃, and keep the reaction temperature React at 40-45°C for 6 hours, and cool to room temperature to obtain ethanolamine sulfate for use.

[0023] (2) Ice analysis

[0024] The obtained ethanolamine sulfate trickle is added to the reactor with direct ice, and the temperature is maintained at -5 to 15°C with direct ice until all is added. The material department analyzes it for use.

[0025] (3) Neutralization

[0026] Adjust the pH of the iced liquid to 7 with hydrogen carbonate.

[0027] (4) Alkali treatment

[0028] Maintain the temperature of the ice leaching solution at -5-15°C, add a 30% mass concentration NaOH solution, adjust the pH to 11.0-12.5, and keep the temperature for 1 hour.

[0029] (5) Neutralization

[0030] Add 30% hydrochloric acid to neutrali...

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PUM

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Abstract

The invention relates to a preparation method for vinyl amine. The method comprises the following steps of: (1) adding oleum into a reactor, then cooling by an outer bath, adding ethanolamine at the temperature below 30 DEG C, heating up to a temperature between 40 and 60 DEG C, maintaining a reaction temperature between 40 and 60 DEG C for 4 to 8 hours, and cooling to a room temperature to obtain ethanolamine sulfuric acid ester; (2) adding the obtained ethanolamine sulfuric acid ester into a reactor with direct ice by trickles, and maintaining the temperature between -5 and 15 DEG C with the direct ice until ester is totally added and partial materials are separated out, and obtaining an ice-out liquid; (3) adjusting pH of the ice-out liquid to 7 with acid catcher; (4) maintaining the temperature of the ice-out liquid between -5 and 15 DEG C, adding 30 mass percent NaOH solution, adjusting pH to between 11.0 and 12.5, keeping the temperature, and reacting; and (5) adding 30 percent hydrochloric acid to neutralize until pH is equal to 7, then spraying, and drying to prepare the vinyl amine.

Description

Technical field [0001] The invention belongs to the field of intermediate products of synthetic dyes, and particularly relates to a preparation method of vinylamine. Background technique [0002] As a new type of dye intermediate, vinylamine is the raw material of ethanolamine and oleum. There are many methods for preparing vinylamine, but the existing methods are expensive. These include: oleum sulfuric acid esterification, thio trioxide esterification, chlorosulfonic acid esterification, sulfamic acid esterification and other methods. However, due to the difficult post-treatment of sulfamic acid esterification, the low conversion rate of thiotrioxide esterification and chlorosulfonic acid esterification, and the dangerous operation, this patent uses the fuming sulfuric acid esterification method. In this method, raw materials are easy to obtain, and the manufacturing process is simple and easy to implement. During the preparation process, because ethanolamine itself has a ce...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/21C07C209/68
Inventor 张兴华郝津来
Owner TIANJIN DEK CHEM